CN105185497A - Preparation method of permanent magnet material - Google Patents
Preparation method of permanent magnet material Download PDFInfo
- Publication number
- CN105185497A CN105185497A CN201510545815.2A CN201510545815A CN105185497A CN 105185497 A CN105185497 A CN 105185497A CN 201510545815 A CN201510545815 A CN 201510545815A CN 105185497 A CN105185497 A CN 105185497A
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- Prior art keywords
- magnet
- rare earth
- earth element
- magnetic
- present
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Links
- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 84
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 58
- 238000000576 coating method Methods 0.000 claims abstract description 46
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000012466 permeate Substances 0.000 claims abstract description 5
- 229910001172 neodymium magnet Inorganic materials 0.000 claims description 52
- 238000004519 manufacturing process Methods 0.000 claims description 36
- 229910045601 alloy Inorganic materials 0.000 claims description 32
- 239000000956 alloy Substances 0.000 claims description 32
- 230000032683 aging Effects 0.000 claims description 27
- 238000005245 sintering Methods 0.000 claims description 27
- 230000008018 melting Effects 0.000 claims description 22
- 238000002844 melting Methods 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 18
- 238000000465 moulding Methods 0.000 claims description 15
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- 239000010453 quartz Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 230000008595 infiltration Effects 0.000 claims description 11
- 238000001764 infiltration Methods 0.000 claims description 11
- 239000000696 magnetic material Substances 0.000 claims description 11
- 238000011112 process operation Methods 0.000 claims description 11
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 8
- 229910052771 Terbium Inorganic materials 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 7
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 7
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052779 Neodymium Inorganic materials 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 5
- 229910052691 Erbium Inorganic materials 0.000 claims description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 4
- 229910052689 Holmium Inorganic materials 0.000 claims description 4
- 229910052765 Lutetium Inorganic materials 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
- 229910052775 Thulium Inorganic materials 0.000 claims description 4
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 4
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 4
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 4
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims description 4
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 4
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 4
- 238000004513 sizing Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 2
- 230000005389 magnetism Effects 0.000 abstract description 6
- 238000007789 sealing Methods 0.000 abstract description 5
- 230000035699 permeability Effects 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 150000002910 rare earth metals Chemical class 0.000 description 10
- 125000004429 atom Chemical group 0.000 description 8
- 238000003825 pressing Methods 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 238000005520 cutting process Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000003801 milling Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 239000003708 ampul Substances 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- -1 rare earth compound Chemical class 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000001962 electrophoresis Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 150000002484 inorganic compounds Chemical class 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 230000003204 osmotic effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- FMGSKLZLMKYGDP-USOAJAOKSA-N dehydroepiandrosterone Chemical class C1[C@@H](O)CC[C@]2(C)[C@H]3CC[C@](C)(C(CC4)=O)[C@@H]4[C@@H]3CC=C21 FMGSKLZLMKYGDP-USOAJAOKSA-N 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 230000005347 demagnetization Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010285 flame spraying Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 238000010902 jet-milling Methods 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/005—Impregnating or encapsulating
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
Abstract
The invention discloses a preparation method of a permanent magnet material. The method comprises a coating procedure and a permeation procedure, wherein a material containing a rare-earth element coats the surface of a permanent magnet; the thickness of the permanent magnet in one direction is at least less than 10mm; the permanent magnet is put into a container for vacuum supply until the intensity of air pressure is less than 10Pa; a channel is sealed; and a sealing device is subjected to heat treatment. By the method disclosed by the invention, the rare-earth element can permeate evenly and the permeability is high. In addition, the method is relatively low in cost; and the coercive force of the permanent magnet material is greatly improved while the residual magnetism is reduced slightly.
Description
Technical field
The present invention relates to a kind of preparation method of permanent magnetic material, especially a kind ofly obtain in low cost mode the preparation method that coercive force increases substantially, remanent magnetism reduces little Nd-Fe-Bo permanent magnet material.
Background technology
Along with the world is to the pay attention to day by day reducing energy resource consumption, energy-saving and emission-reduction have become the emphasis that every country is paid close attention to.Compared with non-magneto, magneto can improve Energy Efficiency Ratio, and in order to reduce energy consumption, at compressor of air conditioner, the fields such as electric automobile hybrid vehicle all adopt neodymium iron boron (Nd-Fe-B) permanent magnetic material to make motor.Because these machine operation temperature are higher, so all require that magnet has higher HCJ, and, in order to increase the magnetic flux density of motor, also require that magnet has higher magnetic energy product.
Adopt traditional neodymium iron boron manufacturing process to be difficult to meet the requirement of high energy product and high HCJ, even if reach such requirement, also need to use a large amount of rare earth β-diketone complex and Tb.Because the reserves of dysprosium (Dy) and terbium (Tb) are in the world limited, a large amount of use Dy and Tb can cause the acceleration of the rise in price of magnet and rare earth resources exhausted.
In order to improve permanent magnetic material performance and reduce the consumption of rare earth, industry has done a lot of work.Such as, CN101404195A discloses a kind of method for the preparation of rare-earth permanent magnet, comprise: provide by the rare earth of 12-17 atom %, the B of 3-15 atom %, the metallic element of 0.01-11 atom %, the O of 0.1-4 atom %, the C of 0.05-3 atom %, the sintered magnet body of the N of 0.01-1 atom % and the Fe composition of surplus, the surface of magnet body is arranged the oxide comprising another kind of rare earth, the powder of fluoride and/or oxyfluoride, and the magnet body that at temperature in a vacuum or in an inert atmosphere below sintering temperature, this powder of heat treatment covers, be absorbed in magnet body to make other rare earths.The feature of the method makes to arrange that the method for the oxide of heavy rare earth or fluoride and/or oxyfluoride heating realizes the object of infiltration by surface, and the shortcoming of the method is the introduction of the material harmful to magnet such as O and F.The more important thing is, the magnet surface of having permeated has the more material being similar to oxide skin, needs to carry out mill processing, causes the waste of magnetic material.
And for example, CN101506919A discloses a kind of manufacture method of permanent magnet, and it can not make the sintered magnet surface deterioration of Nd-Fe-B system, by making Dy efficiently be diffused in Grain-Boundary Phase, effectively improving magnetization and coercive force, not needing subsequent handling.First, in process chamber, the sintered magnet of Nd-Fe-B system and Dy are configured at a certain distance.Then, under reduced pressure process chamber is heated, while making sintered magnet be warmed up to set point of temperature, Dy is evaporated, the Dy atom of evaporation is provided to sintered magnet surface and makes it attachment.Now, by the quantity delivered of control Dy atom pair sintered magnet, before sintered magnet forms Dy layer on the surface, Dy is diffused among the Grain-Boundary Phase of sintered magnet equably.The method feature is that the material of heating containing heavy rare earth forms steam, and shortcoming is equipment manufacturing cost costliness, and evaporation efficiency is low, and the result display of actual contrast, the method is not as the successful of preceding method increase HCJ (Hcj).
CN101615459A discloses a kind of method that rapid-hardening flake grain boundary decision heavy rare earth compound improves sintered NdFeB permanent magnet performance, the method carries out infiltration process before sintering, its shortcoming is when in the process of magnet at high temperature sintering after infiltration, originally the heavy rare earth being enriched to intergranular phase can be diffused into principal phase inside, cause the equalization of heavy rare earth, weak effect.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of permanent magnetic material, the method can significantly improve the infiltration uniformity and the osmotic efficiency of rare earth element.Further object of the present invention is the preparation method providing a kind of permanent magnetic material, and it can make the coercive force of permanent magnetic material greatly improve, but remanent magnetism reduces seldom.
The invention provides a kind of preparation method of permanent magnetic material, comprise following operation:
S2) operation is applied: by the coating substance containing rare earth element on the surface of magnet, wherein, described magnet thickness at least is in one direction below 10mm; With
S3) permeate operation, comprise the steps:
S3-1) by by coating operation S2) magnet that obtains is placed in container, and described container has the passage that can carry out vacuum pumping;
S3-2) by described passage, vacuum pumping is carried out to described container, until the air pressure pressure of described container is lower than 10Pa;
S3-3) in the process continuing to vacuumize by described channel enclosed;
S3-4) magnet be enclosed in described container is heat-treated.
Preparation in accordance with the present invention, preferably, at coating operation S2) in, the described material containing rare earth element is selected from:
A1) simple substance of rare earth element;
A2) containing the alloy of rare earth element;
A3) containing the compound of rare earth element; Or
A4) mixture of above material.
Preparation in accordance with the present invention, preferably, at coating operation S2) in, described rare earth element is selected from least one in praseodymium, neodymium, yttrium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium.
Preparation in accordance with the present invention, preferably, at coating operation S2) in, described magnet thickness at least is in one direction below 5mm.
Preparation in accordance with the present invention, preferably, at infiltration operation S3) in, described container and described passage are quartz material, and the internal diameter of described passage is 3 ~ 15mm.
Preparation in accordance with the present invention, preferably, in step S3-1) in, will at least two by coating operation S2) magnet arrangements that obtains is neat, and with the maximum surface of respective area for contact-making surface, close contact mutually under pressure, is then placed in described container.
Preparation in accordance with the present invention, preferably, in step S3-1) in, the pressure of described pressure effect is at least 5MPa.
Preparation in accordance with the present invention, preferably, in step S3-2) in, by described passage, vacuum pumping is carried out to described container until described container air pressure pressure lower than to container vacuum-pumping to air pressure pressure lower than 5Pa; With
In step S3-4) in, heat treatment temperature is 600 ~ 1200 DEG C; Heat treatment time is 0.5 ~ 10 hour.
Preparation in accordance with the present invention, preferably, described manufacture method also comprises:
S1) magnet manufacturing process: manufacture magnet; With
S4) ageing treatment process: Ageing Treatment is carried out to magnet.
Preparation in accordance with the present invention, preferably, described magnet manufacturing process S1) comprise following operation:
S1-1) melting operation: melting is carried out to neodymium iron boron magnetic body raw material, make the neodymium iron boron magnetic body raw material after melting form foundry alloy, the thickness of described foundry alloy is 0.01 ~ 5mm;
S1-2) powder process operation: by by melting operation S1-1) foundry alloy that obtains is broken into magnetic, and the mean particle size D 50 of described magnetic is less than 20 μm;
S1-3) molding procedure: under the effect of alignment magnetic field, by by powder process operation S1-2) magnetic that obtains is pressed into sintered body, and the density of described base substrate is 3.0g/cm
3~ 5g/cm
3; With
S1-4) sintering circuit: will by molding procedure S1-3) the sintered body sintering sizing that obtains, form magnet; Sintering temperature is 900 ~ 1300 DEG C, and sintering time is 0.5 ~ 10 hour; Magnet density is 6.0g/cm
3~ 9.0g/cm
3.
The present invention, by having material containing rare earth element in the surface-coated of the magnet with specific thicknesses, and after the magnet after coating is adopted specific vacuum treatment, then manufactures Nd-Fe-Bo permanent magnet material after heat treatment and Ageing Treatment.Adopt manufacture method of the present invention that rare earth element can be made to permeate evenly and osmotic efficiency is high.According to the preferred technical scheme of the present invention, manufacture method of the present invention can realize the uniformly penetrating of rare earth element in magnet, thus significantly improves the coercive force of magnet, but remanent magnetism reduces seldom.According to the present invention's preferred technical scheme further, owing to not carrying out Ageing Treatment in the preparation section of magnet, thus save manufacturing cost.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details, but protection scope of the present invention is not limited to this.
" remanent magnetism " of the present invention, refers to that magnetic field intensity on saturation hysteresis loop is the numerical value of magnetic flux density corresponding to zero place, is usually denoted as B
ror M
r, unit is tesla (T) or Gauss (Gs).
" HCJ " of the present invention, refers to the saturation magnetization state from magnet, magnetic field is reduced to zero monotonously and oppositely increases, and magnetic field intensity when making its magnetization be reduced to zero along saturation hysteresis loop, is denoted as H usually
cjor
mh
c, unit is oersted (Oe).
" magnetic energy product " of the present invention, refers to the magnetic flux density (B) of any point on demagnetization curve and the product of corresponding magnetic field intensity (H), is usually denoted as BH.The maximum of BH is called " maximum magnetic energy product ", is usually denoted as (BH)
max, unit is Gauss's oersted (GOe).
Rare earth element of the present invention includes but not limited to praseodymium, neodymium or " heavy rare earth element "; Be preferably " heavy rare earth element "." heavy rare earth element " of the present invention, be also called " yittrium group ", comprise nine kinds of elements such as yttrium (Y), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu).
" inert atmosphere " of the present invention, refers to and does not react with neodymium iron boron magnetic body, and do not affect the atmosphere of its magnetic.In the present invention, described " inert atmosphere " comprises the atmosphere formed by inert gas (helium, neon, argon gas, Krypton, xenon).
" vacuum " of the present invention, refers to Absolute truth reciprocal of duty cycle; Its numerical value is less, represents that vacuum degree is higher.
The equivalent diameter of the largest particles when cumulative distribution is 50% in " mean particle size D 50 " of the present invention expression size distribution curve.
The manufacture method of permanent magnetic material of the present invention comprises coating operation S2) and infiltration operation S3).Preferably, manufacture method of the present invention also comprises magnet manufacturing process S1) and ageing treatment process S4), and magnet manufacturing process S1) coating operation S2) before carry out, ageing treatment process S4) infiltration operation S3) after carry out.
In the present invention, described magnet can be Sintered NdFeB magnet or other magnets, is preferably Sintered NdFeB magnet.Be described for Sintered NdFeB magnet below.
< magnet manufacturing process S1) >
Magnet manufacturing process S1 of the present invention) for the manufacture of Sintered NdFeB magnet.In the present invention, magnet manufacturing process S1) preferably include following operation:
S1-1) melting operation: carry out melting to neodymium iron boron magnetic body raw material, makes the neodymium iron boron magnetic body raw material after melting form foundry alloy;
S1-2) powder process operation: by by melting operation S1-1) foundry alloy that obtains is broken into magnetic;
S1-3) molding procedure: under the effect of alignment magnetic field, by by powder process operation S1-2) magnetic that obtains is pressed into sintered body; With
S1-4) sintering circuit: will by molding procedure S1-3) the sintered body sintering sizing that obtains, form Sintered NdFeB magnet.
According to the preferred embodiment of the present invention, magnet manufacturing process S1) following operation can also be comprised:
S1-5) temper operation: temper is carried out to Sintered NdFeB magnet; And/or
S1-6) cutting action: Sintered NdFeB magnet is cut.
melting operation S1-1)
In order to the foundry alloy preventing neodymium iron boron magnetic body raw material and obtained by it is oxidized, melting operation S1-1 of the present invention) preferably carry out in vacuum or inert atmosphere.At melting operation S1-1) in, neodymium iron boron magnetic body raw material and proportioning thereof are had no particular limits, raw material well known in the art and proportioning can be used.At melting operation S1-1 of the present invention) in, smelting technology preferably adopts casting ingot process or rapid hardening slab technique (StripCasting).Casting ingot process is the neodymium iron boron magnetic body raw material cooled and solidified after melting, and is made into alloy pig (foundry alloy).Rapid hardening slab is the rapid cooled and solidified of neodymium iron boron magnetic body raw material after melting, and is got rid of into alloy sheet (foundry alloy).According to the present invention one preferred embodiment, smelting technology adopts rapid hardening slab technique.Present inventor is surprised to find, and compared to casting ingot process, rapid hardening slab technique can avoid the α-Fe occurring affecting dispersed-powder, and can avoid occurring the rich neodymium phase of lumps, thus is conducive to foundry alloy principal phase Nd
2fe
14the refinement of B crystallite dimension.Rapid hardening slab technique of the present invention is preferably carried out in vacuum smelting fast solidification stove.Alloy sheet of the present invention (foundry alloy) thickness can be 0.01 ~ 5mm, is preferably 0.05 ~ 1mm, is more preferably 0.1 ~ 0.5mm; Oxygen content can be below 2000ppm, is preferably below 1500ppm, is more preferably below 1200ppm.
powder process operation S1-2)
In order to the magnetic preventing foundry alloy and obtained by its fragmentation is oxidized, powder process operation S1-2 of the present invention) preferably carry out in vacuum or inert atmosphere.Flouring technology S1-2 of the present invention) preferably include following operation:
S1-2-1) coarse crushing operation: foundry alloy is broken into the thick magnetic that granularity is larger; With
S1-2-2) abrasive dust operation: by by coarse crushing operation S1-2-1) the thick magnetic that obtains wears into thin magnetic.
In the present invention, by coarse crushing technique S1-2-1) mean particle size D 50 of thick magnetic that obtains can be less than 500 μm, is preferably less than 350 μm, is more preferably 300 ~ 100 μm.In the present invention, by milling process S1-2-2) mean particle size D 50 of thin magnetic that obtains can be less than 20 μm, is preferably less than 10 μm, is more preferably 1 ~ 5 μm.
At coarse crushing operation S1-2-1 of the present invention) in, adopt Mechanical Crushing technique and/or hydrogen decrepitation (HydrogenDecrepitation) that foundry alloy is broken into thick magnetic.Foundry alloy is broken into thick magnetic for using mechanical disruption device by Mechanical Crushing technique.Described mechanical disruption device can be selected from jaw crusher or hammer mill.Hydrogen decrepitation comprises the steps: first to make foundry alloy inhale hydrogen, and the volumetric expansion being caused foundry alloy lattice by foundry alloy and hydrogen reaction makes foundry alloy fragmentation form thick magnetic, then heats described thick magnetic and carries out dehydrogenation.According to the present invention one preferred embodiment, hydrogen decrepitation of the present invention preferably carries out in the broken stove of hydrogen.In hydrogen decrepitation of the present invention, inhaling hydrogen temperature is 50 DEG C ~ 400 DEG C, is preferably 100 DEG C ~ 300 DEG C; Suction hydrogen pressure is 50 ~ 600kPa, is preferably 100 ~ 500kPa; Desorption temperature is 500 ~ 1000 DEG C, is preferably 700 ~ 900 DEG C.
At abrasive dust operation S1-2-2 of the present invention) in, adopt ball-milling technology and/or airflow milling technique (JetMilling) that described thick magnetic is broken into thin magnetic.Described thick magnetic is broken into thin magnetic for adopting mechanical ball mill apparatus by ball-milling technology.Described mechanical ball mill apparatus can be selected from rolling ball milling, vibratory milling or high-energy ball milling.Airflow milling technique is mutually collision and broken after utilizing air-flow that thick magnetic is accelerated.Described air-flow can be nitrogen stream, is preferably High Purity Nitrogen air-flow.N in described High Purity Nitrogen air-flow
2content can at more than 99.0wt%, preferably at more than 99.9wt%.The pressure of described air-flow can be 0.1 ~ 2.0MPa, is preferably 0.5 ~ 1.0MPa, is more preferably 0.6 ~ 0.7MPa.
According to the present invention one preferred embodiment, first, by hydrogen decrepitation, foundry alloy is broken into thick magnetic; Then, by airflow milling technique, described thick magnetic is broken into thin magnetic.
According to another implementation of the invention, powder process operation S1-2) m elt-spun overqu-enching (Magnequench) can be adopted to manufacture magnetic.M elt-spun overqu-enching can use known in the art those, repeat no more here.
molding procedure S1-3)
In order to prevent magnetic oxidized, molding procedure S1-3 of the present invention) preferably carry out in vacuum or inert atmosphere.Magnetic pressing process of the present invention preferably adopts mold pressing pressing process and/or isostatic pressed pressing process.Mold pressing pressing process and isostatic pressed pressing process can adopt known in the art those, repeat no more here.At molding procedure S1-3 of the present invention) in, alignment magnetic field direction and magnetic pressing direction are parallel to each other orientation or mutually vertical orientated.The intensity of alignment magnetic field has no particular limits, and is determined by actual needs.According to the preferred embodiment of the present invention, the intensity of alignment magnetic field is at least 0.5 tesla (T), is preferably at least 0.7T.According to the preferred embodiment of the present invention, the intensity of alignment magnetic field, lower than 3T, is preferably lower than 2.5T.According to one of the present invention preferred embodiment, the intensity of alignment magnetic field is 0.7 ~ 2T.By moulding process S1-3 of the present invention) blank density that obtains can be 3.0g/cm
3~ 5g/cm
3, be preferably 3.5g/cm
3~ 4.5g/cm
3.
sintering circuit S1-4)
In order to prevent sintered body oxidized, sintering circuit S1-4) preferably carry out in vacuum or inert atmosphere.According to the preferred embodiment of the present invention, sintering circuit S1-4) carry out in vacuum sintering furnace.Sintering temperature can be 900 ~ 1300 DEG C, is preferably 1000 ~ 1200 DEG C, is more preferably 1000 ~ 1080 DEG C; Sintering time can be 0.5 ~ 10 hour, is preferably 1 ~ 6 hour.By moulding process S1-4 of the present invention) the Sintered NdFeB magnet density that obtains can be 6.0g/cm
3~ 9.0g/cm
3, be preferably 6.5g/cm
3~ 8.0g/cm
3.
Cutting action S1-5)
At cutting action S1-5 of the present invention) in, cutting technique adopts slice processing technique and/or Wire EDM technique.In the present invention, the thickness cut into by Sintered NdFeB magnet at least is in one direction below 10mm, is preferably the magnet of below 5mm.As preferably, described thickness is below 10mm, and the direction being preferably below 5mm is the direction of orientation of Sintered NdFeB magnet.In the present invention, the thickness cut into by Sintered NdFeB magnet at least is in one direction preferably more than 0.1mm, is more preferably the magnet of more than 1mm.
In the present invention, magnet manufacturing process S1) preferably at coating operation S2) carry out before.At magnet manufacturing process S1) in, can carry out or not carry out Ageing Treatment.In order to cost-saving, preferably at magnet manufacturing process S1) in do not carry out Ageing Treatment.
< applies operation S2) >
Coating operation S2 of the present invention) for will the coating substance of rare earth element be contained on the surface of Sintered NdFeB magnet.Material containing rare earth element of the present invention is selected from:
A1) simple substance of rare earth element;
A2) containing the alloy of rare earth element;
A3) containing the compound of rare earth element; Or
A4) any mixture of above material.
At the alloy (a2) containing rare earth element of the present invention) in, except containing except rare earth element, also containing other metallic element.Preferably, other metallic element described is selected from least one in aluminium, gallium, magnesium, tin, silver, copper and zinc.
Compound (a3) containing rare earth element of the present invention) for containing inorganic compound or the organic compound of rare earth element.Inorganic compound containing rare earth element includes but not limited to the oxide of rare earth element, hydroxide or inorganic acid salt.Organic compound containing rare earth element includes but not limited to containing the acylate of rare earth element, alkoxide or metal complex.According to the present invention one preferred embodiment, the compound containing rare earth element of the present invention is the halide of rare earth element, the fluoride of such as rare earth element, chloride, bromide or iodide.
Contain in the material of rare earth element of the present invention, rare earth element is selected from praseodymium, neodymium or yittrium group (heavy rare earth element), be such as selected from least one in yttrium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium.According to one of the present invention preferred embodiment, described rare earth element is at least one in dysprosium or terbium.
Coating operation S2 of the present invention) coating processes that adopts can adopt the conventional coating processes in this area, such as, adopt wet coating, dry method to apply or its combination applies.
Wet coating of the present invention preferably adopts following coating processes or its combination:
S2-1) substance dissolves containing rare earth element is formed in liquid medium the coating liquid of solution form, utilize the surface of coating liquid to Sintered NdFeB magnet of described solution form to apply; Or
S2-2) material containing rare earth element is dispersed in liquid medium the coating liquid forming suspension or emulsion form, utilizes the surface of the coating liquid of described suspension or emulsion form to Sintered NdFeB magnet to apply; Or
S2-3) coating liquid of the material containing rare earth element is provided, Sintered NdFeB magnet is immersed in described coating liquid, formed the plated film of the material containing rare earth element by chemical plating, plating or electrophoresis on the surface of Sintered NdFeB magnet.
At coating processes S2-1) and S2-2) in, the coating method of coating liquid has no particular limits, and can adopt the conventional coating method in this area, such as dip-coating, brushing, spin coating, spraying, roller coat, silk screen printing or inkjet printing.The liquid medium of coating liquid can be selected from water, organic solvent or its combination.
At coating processes S2-3) in, chemical plating, plating and electrophoresis process have no particular limits, and can adopt this area common process.
Dry method coating of the present invention preferably adopts following coating processes or its combination:
S2-4) material containing rare earth element is made powder, by the surface of described powder coated in Sintered NdFeB magnet; Or
S2-5) by gas-phase deposition, by the electrodeposition substance containing rare earth element on the surface of Sintered NdFeB magnet.
Coating processes S2-4 of the present invention) preferably adopt at least one in flame spraying (plasma spraying), fluidized bed process, electrostatic powder spraying, electrostatic flu, electrostatic powder succusion.According to one of the present invention preferred embodiment, operation S2 is applied) adopt above-mentioned coating processes S2-4) carry out dry method coating.
Coating processes S2-5 of the present invention) preferably adopt at least one in chemical vapour deposition (CVD) (chemicalvapordeposition, be called for short CVD) and physical vapour deposition (PVD) (physicalvapordeposition, abbreviation PVD).
< permeates operation S3) >
Infiltration operation S3 of the present invention) preferably include following steps:
S3-1) by by coating operation S2) Sintered NdFeB magnet that obtains is placed in container, and described container has the passage that can carry out vacuum pumping;
S3-2) by described passage, vacuum pumping is carried out to described container, until the air pressure pressure of described container is lower than 10Pa;
S3-3) in the process continuing to vacuumize by described channel enclosed;
S3-4) Sintered NdFeB magnet be enclosed in described container is heat-treated.
In the present invention, described container and passage all adopt exotic material to make, to avoid melting in follow-up heat treatment and/or Ageing Treatment.Preferably, described exotic material is quartz.Preferably, the internal diameter of described passage is 3 ~ 15mm, is preferably 5 ~ 12mm, is more preferably 6 ~ 10mm.Adopt such structure, be more conducive to the " locked in " operation to passage.
In step S3-1) in, will at least two by coating operation S2) the Sintered NdFeB magnet marshalling that obtains, and with the maximum surface of respective area for contact-making surface, close contact mutually under pressure, is then placed in described container.The pressure of pressure effect of the present invention can be at least 5MPa, is preferably 5 ~ 1000MPa, is more preferably 50 ~ 500MPa.
In step S3-2) in, the air pressure pressure of described container can lower than 5Pa, preferably lower than 1Pa, preferred lower than 0.0001Pa further.Can be sealing by the mode of described channel enclosed.
In step S3-4) in, heat treatment temperature can be 600 ~ 1200 DEG C, is preferably 800 ~ 1000 DEG C; Heat treatment time is 0.5 ~ 10 hour, is preferably 2 ~ 8 hours, is more preferably 3 ~ 6 hours.
< ageing treatment process S4) >
Ageing treatment process S4 of the present invention) for carrying out Ageing Treatment to Sintered NdFeB magnet.In the present invention, the temperature of Ageing Treatment can be 300 ~ 900 DEG C, is preferably 400 ~ 600 DEG C; The time of Ageing Treatment can be 0.5 ~ 10 hour, is preferably 1 ~ 6 hour, is more preferably 2 ~ 5 hours.According to the preferred embodiment of the present invention, ageing treatment process S4) at infiltration operation S3) after carry out.
embodiment 1
S1) magnet manufacturing process:
S1-1) melting operation: by weight percentage, Nd according to 23.5%, the Pr of 5.5%, 2% Dy, 1% B, 1% Co, Cu, the Zr of 0.08% of 0.1%, the Fe preparation raw material of the Ga of 0.1% and surplus, raw material is placed in vacuum smelting fast solidification stove and carries out melting, make the alloy sheet that average thickness is 0.3mm;
S1-2) powder process operation: to by melting operation S1-1 in the broken stove of hydrogen) alloy sheet that obtains carries out suction hydrogen and Dehydroepiandrosterone derivative, make described alloy sheet crushing-type become particle diameter to be the thick magnetic of 300 μm, described thick magnetic is worn into the thin magnetic that mean particle size D 50 is 4.2 μm in the vehicular airflow milling of nitrogen;
S1-3) molding procedure: in the moulding press of nitrogen protection, applies 1.8T magnetic field to by powder process operation S1-2) the thin magnetic oriented moulding that obtains forms sintered body, and compact density is 4.3g/cm
3;
S1-4) sintering circuit: by by molding procedure S1-3) sintered body that obtains puts into vacuum sintering furnace high temperature sintering and forms Sintered NdFeB magnet, vacuum degree in described vacuum sintering furnace is about 0.1Pa, sintering temperature is 1050 DEG C, sintering time is 5 hours, and the density of the Sintered NdFeB magnet obtained reaches 7.6g/cm
3, be of a size of 50mm × 40mm × 30mm;
S1-5) cutting action:
By by sintering circuit S1-4) Sintered NdFeB magnet that obtains cuts into the magnet being of a size of 38mm × 23.5mm × 4mm.
S2) operation is applied:
Terbium powder coated will be fluoridized by magnet manufacturing process S1) Sintered NdFeB magnet surface after the cutting that obtains.
S3) operation is permeated:
S3-1) by by coating operation S2) Sintered NdFeB magnet that obtains is placed in quartz container, and the quartz ampoule sealing that this quartz container is 7mm by a diameter is communicated with;
S3-2) by described quartz ampoule, air pressure pressure is evacuated to lower than 1Pa to quartz container;
S3-3) continue to vacuumize lower to quartz ampoule sealing;
S3-4) heat-treat Sintered NdFeB magnet, heat treatment temperature is 900 DEG C, and heat treatment time is 5 hours;
S4) ageing treatment process:
Under vacuum, to by infiltration operation S3) Sintered NdFeB magnet that obtains carries out Ageing Treatment, and aging temperature is 500 DEG C, and aging time is 3 hours.
embodiment 2
Step S3-1 except by embodiment 1) be revised as except following steps, other conditions are identical with embodiment 1: will by applying operation S2) Sintered NdFeB magnet that obtains is along the direction marshalling of thickness 4 millimeters, by fixture, the Sintered NdFeB magnet two ends after marshalling are implemented to the pressure of 500MPa, then be placed in quartz container by the Sintered NdFeB magnet of this enforcement pressure, the quartz ampoule sealing that this quartz container is 7mm by a diameter is communicated with.
comparative example 1
To S1-4 in embodiment 1) Sintered NdFeB magnet that obtains of sintering circuit carries out Ageing Treatment, and aging temperature is 500 DEG C, and aging time is 3 hours.
comparative example 2
To S2 in embodiment 1) apply the Sintered NdFeB magnet that operation obtains and be positioned in the graphite under normal pressure, heat-treat, heat treatment temperature is 900 DEG C, and heat treatment time is 5 hours; Then carry out Ageing Treatment, aging temperature is 500 DEG C, and aging time is 3 hours.
experimental example 1
Sintered NdFeB magnet embodiment 1-2, comparative example 1-2 obtained cuts into the magnet of 9*9*4mm respectively, measures its " remanent magnetism " (B
r) and " HCJ " (H
cj), experimental result is in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Comparative example 1 | Comparative example 2 | |
| Br(kGs) | 13.71 | 13.70 | 13.82 | 13.75 |
| Hcj(kOe) | 26.52 | 27.48 | 18.25 | 25.85 |
The present invention is not limited to above-mentioned execution mode, and when not deviating from flesh and blood of the present invention, any distortion that it may occur to persons skilled in the art that, improvement, replacement all fall into scope of the present invention.
Claims (10)
1. a preparation method for permanent magnetic material, is characterized in that, comprises following operation:
S2) operation is applied: by the coating substance containing rare earth element on the surface of magnet, wherein, described magnet thickness at least is in one direction below 10mm; With
S3) permeate operation, comprise the steps:
S3-1) by by coating operation S2) magnet that obtains is placed in container, and described container has the passage that can carry out vacuum pumping;
S3-2) by described passage, vacuum pumping is carried out to described container, until the air pressure pressure of described container is lower than 10Pa;
S3-3) in the process continuing to vacuumize by described channel enclosed;
S3-4) magnet be enclosed in described container is heat-treated.
2. preparation method according to claim 1, is characterized in that, at coating operation S2) in, the described material containing rare earth element is selected from:
A1) simple substance of rare earth element;
A2) containing the alloy of rare earth element;
A3) containing the compound of rare earth element; Or
A4) mixture of above material.
3. preparation method according to claim 2, is characterized in that, at coating operation S2) in, described rare earth element is selected from least one in praseodymium, neodymium, yttrium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium.
4. manufacture method according to claim 1, is characterized in that, at coating operation S2) in, described magnet thickness at least is in one direction below 5mm.
5. manufacture method according to claim 1, is characterized in that, at infiltration operation S3) in, described container and described passage are quartz material, and the internal diameter of described passage is 3 ~ 15mm.
6. manufacture method according to claim 1, it is characterized in that, in step S3-1) in, will at least two by coating operation S2) magnet arrangements that obtains is neat, and with the maximum surface of respective area for contact-making surface, mutual close contact, is then placed in described container under pressure.
7. manufacture method according to claim 6, is characterized in that, in step S3-1) in, the pressure of described pressure effect is at least 5MPa.
8. manufacture method according to claim 1, is characterized in that,
In step S3-2) in, by described passage, vacuum pumping is carried out to described container until described container air pressure pressure lower than to container vacuum-pumping to air pressure pressure lower than 5Pa; With
In step S3-4) in, heat treatment temperature is 600 ~ 1200 DEG C; Heat treatment time is 0.5 ~ 10 hour.
9. manufacture method according to claim 1, is characterized in that, described manufacture method also comprises:
S1) magnet manufacturing process: manufacture magnet; With
S4) ageing treatment process: Ageing Treatment is carried out to magnet.
10. manufacture method according to claim 9, is characterized in that, described magnet manufacturing process S1) comprise following operation:
S1-1) melting operation: melting is carried out to neodymium iron boron magnetic body raw material, make the neodymium iron boron magnetic body raw material after melting form foundry alloy, the thickness of described foundry alloy is 0.01 ~ 5mm;
S1-2) powder process operation: by by melting operation S1-1) foundry alloy that obtains is broken into magnetic, and the mean particle size D 50 of described magnetic is less than 20 μm;
S1-3) molding procedure: under the effect of alignment magnetic field, by by powder process operation S1-2) magnetic that obtains is pressed into sintered body, and the density of described base substrate is 3.0g/cm
3~ 5g/cm
3; With
S1-4) sintering circuit: will by molding procedure S1-3) the sintered body sintering sizing that obtains, form magnet; Sintering temperature is 900 ~ 1300 DEG C, and sintering time is 0.5 ~ 10 hour; Magnet density is 6.0g/cm
3~ 9.0g/cm
3.
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| US15/060,188 US10269488B2 (en) | 2015-08-28 | 2016-03-03 | Preparation of permanent magnet material |
| JP2016042722A JP6276306B2 (en) | 2015-08-28 | 2016-03-04 | Method for manufacturing permanent magnet material |
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| CN105551789A (en) * | 2016-02-04 | 2016-05-04 | 宁波韵升股份有限公司 | Manufacturing method of rare earth permanent magnet |
| CN106409497A (en) * | 2016-08-31 | 2017-02-15 | 浙江东阳东磁稀土有限公司 | Grain boundary diffusion method for neodymium-iron-boron magnet |
| CN107658087A (en) * | 2016-07-25 | 2018-02-02 | Tdk株式会社 | R T B systems sintered magnet |
| WO2018192346A1 (en) * | 2017-04-19 | 2018-10-25 | 安泰科技股份有限公司 | Method for preparing rare earth permanent magnet material |
| CN109014191A (en) * | 2018-07-23 | 2018-12-18 | 沈阳中北真空技术有限公司 | A kind of rare earth permanent magnet vacuum heat treatment furnace and rare earth permanent magnet heat treatment method |
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| CN109935462A (en) * | 2019-03-12 | 2019-06-25 | 宁波雄海稀土速凝技术有限公司 | The preparation method and its neodymium iron boron magnetic body of grain boundary decision heavy rare earth neodymium iron boron magnetic body |
| CN111554502A (en) * | 2020-04-29 | 2020-08-18 | 南京理工大学 | Method for preparing high-coercivity sintered neodymium-iron-boron through pressurization diffusion heat treatment |
| CN113394017A (en) * | 2021-06-10 | 2021-09-14 | 北京工业大学 | Method for sintering neodymium iron boron by electroplating electrophoresis in cooperation with deposition diffusion |
| CN113394017B (en) * | 2021-06-10 | 2023-11-03 | 北京工业大学 | Method for diffusion sintering of neodymium iron boron through electroplating and electrophoresis collaborative deposition |
Also Published As
| Publication number | Publication date |
|---|---|
| EP3043364B1 (en) | 2018-07-11 |
| JP2016129249A (en) | 2016-07-14 |
| US10269488B2 (en) | 2019-04-23 |
| EP3043364A1 (en) | 2016-07-13 |
| US20170062127A1 (en) | 2017-03-02 |
| CN105185497B (en) | 2017-06-16 |
| JP6276306B2 (en) | 2018-02-07 |
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